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目的建立同时测定玉屏风汤中黄芪甲苷、白术内酯-Ⅰ和升麻苷含量的高效液相色谱-质谱法(HPLC-MS)。方法采用Hedera ODS-2(2.0 mm×150 mm,5μm)色谱柱,流动相为甲醇∶水(68∶32),流速为0.2 ml/min;电喷雾电离(ESI+),选择性离子监测(SIM)质荷比为807.50、287.05、469.05的离子对,内标为替米沙坦。结果 3种成分含量的线性范围和相关系数分别为:黄芪甲苷0.015 62～0.5μg/ml(r=0.999 7),白术内酯-Ⅰ0.005 859～0.187 5μg/ml(r=0.999 7),升麻苷0.031 25～8μg/ml(r=0.996 5)。平均回收率分别为:95.47%、101.94%和103.70%,RSD分别为:2.47%、2.20%和1.64%。结论本研究建立的HPLC-MS法方便、快捷、稳定,可同时测定玉屏风汤中3种主要成分的含量,结果准确可靠,可为玉屏风汤体内药动学研究提供依据。
OBJECTIVE To establish a HPLC-MS method for the simultaneous determination of astragaloside IV, atractyloside-I and aconitine in Yupingfeng decoction. Methods The mobile phase was Hedera ODS-2 (2.0 mm × 150 mm, 5 μm). The mobile phase consisted of methanol and water (68:32) at a flow rate of 0.2 ml / min. Electrospray ionization (ESI) ) Mass-to-charge ratio of 807.50,287.05,469.05 ion pair, the internal standard for telmisartan. Results The linear range of the three components and the correlation coefficients were as follows: Astragaloside 0.015 62-0.5 μg / ml (r = 0.999 7), Atractylodisolone I0.005 859-0.1875 μg / ml (r = 0.999 7) , Supranoside 0.031 25 ~ 8μg / ml (r = 0.996 5). The average recoveries were 95.47%, 101.94% and 103.70%, respectively, with RSDs of 2.47%, 2.20% and 1.64%, respectively. Conclusion The HPLC-MS method established in this study is convenient, rapid and stable. The content of three main components in Yupingfeng Decoction can be determined simultaneously. The results are accurate and reliable, which can provide the basis for pharmacokinetic study of Yupingfeng Decoction in vivo.